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试验对草鱼肌肉的提取、浓缩、净化等环节进行了筛选,以甲磺酸达氟沙星作内标物,对流动相、检测器和检测波长等色谱条件进行了选择与优化,在国标方法的基础上,建立了草鱼肌肉组织中诺氟沙星、恩诺沙星和环丙沙星HPLC-FLD多残留检测方法.结果显示,以磷酸-乙腈作提取液,55℃真空旋转蒸发浓缩,正己烷脱脂净化,磷酸-乙腈作流动相,配合荧光检测器(激发波长280nm,发射波长450nm),在0.01～10μg/g范围内线性良好,回收率为79.89%～99.45%,变异系数在7%以内,检测限均为0.006μg/g.为开展上述药物在草鱼中的残留检测以及残留消除规律的研究奠定了基础.
In the experiment, the extraction, concentration and purification of grass carp muscle were screened, and the selection and optimization of the chromatographic conditions such as mobile phase, detector and detection wavelength with danofloxacin mesylate as internal standard were carried out. , A HPLC-FLD multi-residue method for the determination of norfloxacin, enrofloxacin and ciprofloxacin in muscle tissue of grass carp was established.The results showed that the extract was concentrated by rotary evaporation at 55 ℃ with phosphoric acid-acetonitrile, The calibration curve was linear with the concentration of 0.01 ~ 10μg / g and the recovery was 79.89% ~ 99.45% with the fluorescence detector (excitation wavelength 280nm, emission wavelength 450nm) %, The detection limit is 0.006μg / g, which lays the foundation for the research on the residual detection and residual elimination of the above drugs in grass carp.